HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalic Acid → 3-(4-Trifluoromethylphenoxy)-N-methyl-1-azetidinecarboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | Methyl Isocyanate | HCID 12228 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 3-[4-(Trifluoromethyl)phenoxy]azetidine | HCID 12812499 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | 3-(4-Trifluoromethylphenoxy)-N-methyl-1-azetidinecarboxamide | HCID 13420166 | — |
Reaction Steps
The oxalic acid salt of 3-(4-trifluoromethylphenoxy) azetidine (13.0 g., 0.042 mole) was partitioned between 50 ml. of benzene and 50 ml. of potassium hydroxide solution. The benzene layer was dried over calcium sulfate and filtered, and to the stirring dried benzene solution was added 2.6 g. (0.046 mole) of methyl-isocyanate. Stirring was continued overnight. The mixture was concentrated at reduced pressure and the solid residue was recrystallized from a mixture of isopropyl ether-ethyl acetate. The product weighed 7.5 g. (65%) and melted at 154°-157° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04226861 |
| Source dataset | uspto-grants-1980_10 |
| ORD ID | ord-05ba8cda715a4cb3864f6eec80ea4e74 |
| Source note | uspto-grants-1980_10 |